EP0595175B1 - Vorrichtung zur Versorgung von CVD-Beschichtungseinrichtungen - Google Patents

Vorrichtung zur Versorgung von CVD-Beschichtungseinrichtungen Download PDF

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Publication number
EP0595175B1
EP0595175B1 EP93116937A EP93116937A EP0595175B1 EP 0595175 B1 EP0595175 B1 EP 0595175B1 EP 93116937 A EP93116937 A EP 93116937A EP 93116937 A EP93116937 A EP 93116937A EP 0595175 B1 EP0595175 B1 EP 0595175B1
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EP
European Patent Office
Prior art keywords
coating
intermediate reservoir
gas
control device
mass flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP93116937A
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German (de)
English (en)
French (fr)
Other versions
EP0595175A1 (de
Inventor
Hans-Joachim Bittner
Hans-Jürgen Klein
Thomas Küpper
Ewald Mörsen
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Schott AG
Original Assignee
Carl Zeiss AG
Schott Glaswerke AG
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Publication date
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Publication of EP0595175A1 publication Critical patent/EP0595175A1/de
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials

Definitions

  • the invention relates to a device for supplying at least one CVD coating device with coating gas with at least one storage container for the coating material and a piping system between the storage container and the coating device, mass flow controllers and / or valves being arranged in the piping system.
  • Cold light mirrors can be produced, for example, by applying an alternating sequence of two layers with different compositions (20 to 40 layers in total) and different layer thicknesses. It is important here that a rapid change from one gas mixture to the other is possible, so that the total time for the complete coating of the substrates can be kept as short as possible for economic reasons. In addition, because of the high cost of the layer-forming gases, an economical use should be sought, ie the gases should be converted as completely as possible into the layer material without a part flowing away unused and having to be disposed of.
  • JP-A-02-290977 a gas generator is known which is not based on the principle of direct evaporation, but on the carrier gas principle. Different carrier gases are fed through two feed lines to two sublimation baths in which there are further substances. After sublimation, the gases enter a mixing chamber and from there to the reaction chamber where the coating is carried out. This involves precise temperature control.
  • EP 0 018 068 describes a system for the controlled supply of vapors of liquids with low vapor pressure to a system for the production of preforms for optical fibers according to a CVD process.
  • the production time of a preform is in the hour range, so that changes in the gas composition only have to be made slowly. This is why the setting times of the mass flow controllers for the coating duration are not important. Since the reaction gas only flows when it is coated, the problem of economical use of these gases does not arise.
  • the connection line to the coating device must be interrupted, so that the respective service life of the system is limited by the capacity of the storage container.
  • the object of the present invention is a device for the uniform supply of CVD coating devices with coating gases, which allows a quick change of the coating gases with economical use without gas losses and ensures a continuous supply without interruption.
  • This device contains a large-volume intermediate store between the storage container and the coating device (s). In this case, there are at most only small pressure differences in the feed lines to the individual coating devices, which quickly compensate for one another.
  • Another advantage is that the gas is immediately available in the intermediate storage and is therefore independent of the gas source or sources of the storage container and their conditions. Even if the gas supply from the storage container to the intermediate store should be interrupted or disrupted, the coating device can continue to be supplied with gas for a certain time without the coating process having to be interrupted. In particular, if at least two storage containers are provided, continuous operation is ensured because the replacement of the respectively empty storage container can take place without time pressure, since the other (filled) storage container maintains the supply of the intermediate storage.
  • the volume of the intermediate store is chosen so large that only a predetermined maximum pressure change occurs in the intermediate store when gas is withdrawn.
  • M is the total mass flow of the coating gas in mbar. denotes l / s and ( ⁇ p / p) • e.g. is the specified relative pressure change per second in the buffer.
  • p z denotes the pressure in the intermediate store in mbar, p z being greater than the process pressure in the coating device.
  • the requirement for the volume of the buffer store is to be clarified.
  • a plasma pulse CVD process was used to coat domes with a TiO2 layer.
  • the coating parameters were as follows: Period duration: 15 msec Calotte volume: 50 ml Process pressure: 1 mbar TiCl4 pressure in the buffer: 50 mbar Temperature in the buffer: 50 ° C Composition of the coating gas: 2% TiCl4 and 98% O2 Number of domes to be coated simultaneously: 52
  • control valves and / or mass flow controllers which are arranged between the storage container and the intermediate storage device should have a response time of ⁇ 1 sec.
  • the intermediate store has a pressure meter and a temperature sensor, of which the temperature sensor is connected to a control device.
  • the temperature is kept at a predetermined constant value by a temperature control device connected to the first control device.
  • the temperature is preferably between 30 and 200 ° C.
  • the pressure gauge is connected to a further control device which keeps the pressure of the gas contained in the intermediate store between 20 and 1000 mbar.
  • the intermediate store can contain the layer former material in the gaseous state or also in the liquid and gaseous state in thermal equilibrium.
  • the intermediate store is connected to at least one storage vessel in which the layer-forming gas is generated.
  • TiO2 and SiO2 layers are applied alternately by means of a plasma CVD process.
  • Mixtures of oxygen and the layer former hexamethyldisiloxane (HMDSO) on the one hand and oxygen and the layer former material titanium tetrachloride (TiCl4) on the other hand can be used as coating gases.
  • HMDSO and TiCl4 are liquid at room temperature and have a vapor pressure of about 43 and 13 mbar, respectively.
  • Preferably two identical storage containers are connected to an intermediate store. If necessary, heated gas is transferred from the first storage container to the Buffer is released, while the refilling, degassing of liquids and heating take place in the second vessel.
  • the temperature of the liquid is set, for example, by heating the storage container to such a value that the vapor pressure of the liquids as the admission pressure for commercially available mass flow controllers is sufficiently high, which are arranged between the storage container and the intermediate store.
  • a pressure of 50 to 100 mbar can be regarded as sufficient. For TiCl4 and HMDSO this corresponds to a temperature of 50 to 60 or 30 to 45 ° C.
  • the storage containers preferably contain temperature sensors for thermostatting and also fill level sensors which are connected to a control device. This switches the valves of the storage containers so that constant gas generation is guaranteed. If the fill level has dropped below a limit value, the valve flow is switched over to the filled and ready-to-use reserve reservoir - practically uninterrupted for the steam flow.
  • the containers can either be filled on site or filled storage containers can be connected elsewhere.
  • a suitable gas flushing system prevents contamination of critical surfaces.
  • the pressure gauge is electrically connected to a control valve or mass flow controller arranged in the pipeline between the storage container and the intermediate store via a control device.
  • a control valve or mass flow controller arranged in the pipeline between the storage container and the intermediate store via a control device. This is an arrangement for keeping the pressure in the Temporary storage created. If layering gas is removed from the intermediate storage device, the pressure drops below the predetermined limit value. Then, layer-forming gas is supplied from the storage container via the control valve or the mass flow controller until the target pressure in the intermediate store is reached.
  • This embodiment offers the advantage that no layer-forming gas has to be discarded in the coating breaks.
  • the intermediate store contains the liquid layer-forming material and the corresponding gas in thermal equilibrium, the temperature being regulated to a desired value
  • the intermediate store has a fill level meter, which communicates with a valve or mass flow controller arranged in the pipeline between the reservoir and the intermediate store a control device is electrically connected.
  • the level meter has limit switches so that the level can be controlled between two levels. If the fill level falls below a predetermined limit value, coating material is refilled in liquid form from the storage container via the valve or the mass flow controller. Pressure control as in the previously described embodiment is then not necessary.
  • the buffer store is connected to a gas recovery station.
  • a valve is arranged in the pipeline between the gas recovery station and the intermediate store, which valve is electrically connected to the pressure gauge of the intermediate store via a control device.
  • the gas continuously flowing in from the storage container or containers would lead to an undesirable pressure increase in the intermediate storage during the coating breaks. This increase in pressure is registered by the pressure gauge, which opens the valve between the gas recovery station and the intermediate store via the control device, so that the excess gas can flow into the gas recovery station during the coating breaks.
  • the recovery vessel of the gas recovery station is at a lower temperature than the intermediate store and is held there so that the superfluous material condenses there and the recovery vessel acts as a cryopump and therefore no additional pump is required for pumping.
  • the condensed liquid is highly pure and can be reused for coating.
  • the pipeline arranged between the storage container and the intermediate store is connected to the gas recovery station via a valve.
  • the pressure gauge of the intermediate store and the valve in the pipeline leading to the gas recovery station are connected to the control device.
  • the gas also flows out of the storage container continuously and leads to an increase in pressure in the intermediate storage during the coating breaks, which is detected by the pressure gauge.
  • the valve in the to the Gas recovery station leading pipeline opened so that the excess gas can flow through the buffer into the gas recovery station without a detour.
  • the pressure gauge and the temperature sensor can be electrically connected to a control device which is connected to the coating device and controls the coating duration or the mass flow of the coating gases.
  • a control device which is connected to the coating device and controls the coating duration or the mass flow of the coating gases.
  • FIG. 1 schematically shows a device with an intermediate store 9, to which two storage containers 1 and 2 are connected. These storage containers 1 and 2 have limit switches 22, 23 which are connected to a common control device 26. Furthermore, the storage containers 1 and 2 are equipped with temperature sensors 24 and 25, which are also connected to the control device 26.
  • the two storage containers 1 and 2 are connected via pipes 3 and 4 to a main line 7 which opens into the intermediate store 9.
  • Valves 5 and 6 are provided in the pipes 3 and 4 so that the connection to the intermediate store 9 can be interrupted when an empty storage container 1, 2 is replaced.
  • a mass flow controller 8 arranged, which can also be replaced by a control valve. This mass flow controller ensures that the amount of gas flowing in from the reservoir 1 or 2 is kept at a desired value.
  • the intermediate store 9 is equipped with a pressure gauge 14 and a temperature sensor 15. The latter is connected to a control device 21 which is connected to a temperature control device 19 for the intermediate store 9, so that it can be controlled to a desired temperature T2> T1.
  • Pipelines 10, 11 lead from the buffer store 9 to the coating devices 12 and 13.
  • Each coating device 12, 13 can have several coating stations, the gas mass flows being divided by a symmetrical pipe system, optionally provided with means for adjusting the flow resistance, so that the flow resistance between the intermediate store and each coating station and thus the distribution of the gas is as uniform as possible. If the arrangement is to supply coating stations of different sizes simultaneously (exceptionally), then only the flow resistances of the pipelines leading to these need to be adjusted.
  • the symmetrical pipe systems and valves arranged between the intermediate store 9 and the coating stations are not shown in FIG. 1.
  • To the Coating devices 12, 13 are connected to further buffers (not shown) with the associated devices for other layer-forming gases.
  • the pressure meter 14 is connected to a control device 16 which is connected to the mass flow controller 8.
  • the control device 16 When the gas flows from the intermediate store 9 into the coating devices 12 and 13 for coating, the pressure in the intermediate store 9 falls below a predetermined target value, which is measured by the pressure meter 14.
  • a corresponding signal from the control device 16 then opens the mass flow controller 8 or the valve 8 in the main line 7, so that gas can flow in from the respectively active storage container 1 or 2 until the predetermined target value is reached again.
  • FIG. 1 Another embodiment is shown in FIG.
  • the pressure meter 14 and the temperature sensor 15 are connected to a control device 20 which is electrically connected to the coating devices 12 and 13.
  • This control device can also be used in conjunction with the embodiments shown in FIG. 1, FIG. 3, 4 or 5.
  • the components of the device shown in FIG. 1, 3, 4 or 5 were therefore omitted in FIG. 2. If temperature and pressure fluctuations should occur in the intermediate store 9, which could negatively influence the coating in the coating devices 12 and 13, the coating duration and the mass flow in the coating devices 12 and 13 are controlled accordingly by the control device 20, so that even the smallest Fluctuations can be compensated. With this device, on the one hand, a fine adjustment of the layer thickness is possible, on the other hand, there is a further safety reserve against accidents.
  • FIG. 3 shows an arrangement with a gas recovery station 30.
  • the intermediate store 9 is connected via a pipeline 31, in which a throttle 28 and a valve 29 are arranged, to the gas recovery station 30, which is at a temperature T 3 lower than the temperature T 2 of the intermediate store.
  • the pressure gauge 14 is connected to the valve 29 via a control device 27. If the pressure in a coating pause in the intermediate store 9 rises above a predetermined desired value, this is measured by the pressure meter 14, whereupon the valve 29 is opened so that excess layering gas can flow into the gas recovery station 30 and condense.
  • the throttle 28 serves to ensure that the drain from the buffer 9 is free of bumps.
  • FIG. 4 schematically shows an arrangement with respect to the gas recovery station 30 that has been changed compared to the arrangement in FIG. 3.
  • the pipe 31 leading to the gas recovery station 30 opens into the main pipe 7, namely between the mass flow controller 8 and a valve 32.
  • a valve 33 is arranged in the pipe 31 and is connected to the pressure meter 14 via the control device 27. If the pressure in the intermediate store 9 rises above the predetermined target value during a coating break, the control device 27 the valve 32 is closed and the valve 33 is opened, so that the gas flowing in continuously from the storage container 1 or 2 is deflected into the gas recovery station 30.
  • the intermediate store 9 contains the layer former material in both liquid and gaseous form (FIG. 5)
  • the intermediate store 9 is equipped with a level meter 17, which is connected to the control device 16 as an alternative to the pressure meter. If the liquid level in the intermediate store 9 drops below a certain value, this is detected by the level meter 17, whereupon a valve 34 is opened so that liquid layering material can flow from the reservoir 1 into the intermediate store 9.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
EP93116937A 1992-10-28 1993-10-20 Vorrichtung zur Versorgung von CVD-Beschichtungseinrichtungen Expired - Lifetime EP0595175B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4236324 1992-10-28
DE4236324A DE4236324C1 (sv) 1992-10-28 1992-10-28

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EP0595175A1 EP0595175A1 (de) 1994-05-04
EP0595175B1 true EP0595175B1 (de) 1996-02-14

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EP (1) EP0595175B1 (sv)
CA (1) CA2106734C (sv)
DE (2) DE4236324C1 (sv)

Cited By (2)

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US6136725A (en) * 1998-04-14 2000-10-24 Cvd Systems, Inc. Method for chemical vapor deposition of a material on a substrate
US6296711B1 (en) 1998-04-14 2001-10-02 Cvd Systems, Inc. Film processing system

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US5480488A (en) 1996-01-02
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DE4236324C1 (sv) 1993-09-02
DE59301634D1 (de) 1996-03-28

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